US10800689B2 - Magnetic nanoparticle microbial composite with core-shell structure, preparation method thereof, and its application in the treatment of azo dyes - Google Patents
Magnetic nanoparticle microbial composite with core-shell structure, preparation method thereof, and its application in the treatment of azo dyes Download PDFInfo
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- US10800689B2 US10800689B2 US16/164,060 US201816164060A US10800689B2 US 10800689 B2 US10800689 B2 US 10800689B2 US 201816164060 A US201816164060 A US 201816164060A US 10800689 B2 US10800689 B2 US 10800689B2
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- ferroferric oxide
- shell structure
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- 239000002122 magnetic nanoparticle Substances 0.000 title claims abstract description 60
- 239000011258 core-shell material Substances 0.000 title claims abstract description 55
- 239000002131 composite material Substances 0.000 title claims abstract description 38
- 230000000813 microbial effect Effects 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000000987 azo dye Substances 0.000 title abstract description 8
- 239000002105 nanoparticle Substances 0.000 claims abstract description 51
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims abstract description 50
- 244000005700 microbiome Species 0.000 claims abstract description 35
- QMKYBPDZANOJGF-UHFFFAOYSA-N benzene-1,3,5-tricarboxylic acid Chemical compound OC(=O)C1=CC(C(O)=O)=CC(C(O)=O)=C1 QMKYBPDZANOJGF-UHFFFAOYSA-N 0.000 claims abstract description 26
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 22
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 21
- CWERGRDVMFNCDR-UHFFFAOYSA-N thioglycolic acid Chemical compound OC(=O)CS CWERGRDVMFNCDR-UHFFFAOYSA-N 0.000 claims description 20
- 239000000243 solution Substances 0.000 claims description 17
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 10
- 239000001632 sodium acetate Substances 0.000 claims description 10
- 235000017281 sodium acetate Nutrition 0.000 claims description 10
- 239000001509 sodium citrate Substances 0.000 claims description 10
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 8
- 230000035484 reaction time Effects 0.000 claims description 7
- 239000007853 buffer solution Substances 0.000 claims description 4
- 238000012986 modification Methods 0.000 claims description 4
- 230000004048 modification Effects 0.000 claims description 4
- 229940057527 ferric sodium citrate Drugs 0.000 claims description 3
- 239000000975 dye Substances 0.000 abstract description 14
- 230000000694 effects Effects 0.000 abstract description 12
- 238000001179 sorption measurement Methods 0.000 abstract description 10
- 238000007885 magnetic separation Methods 0.000 abstract description 5
- 238000001338 self-assembly Methods 0.000 abstract description 3
- 230000015556 catabolic process Effects 0.000 description 10
- 238000006731 degradation reaction Methods 0.000 description 10
- 238000000034 method Methods 0.000 description 7
- 238000010586 diagram Methods 0.000 description 4
- 230000007613 environmental effect Effects 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 229910021642 ultra pure water Inorganic materials 0.000 description 3
- 239000012498 ultrapure water Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 238000003917 TEM image Methods 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 238000006065 biodegradation reaction Methods 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- ARCGXLSVLAOJQL-UHFFFAOYSA-N trimellitic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C(C(O)=O)=C1 ARCGXLSVLAOJQL-UHFFFAOYSA-N 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 238000010170 biological method Methods 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011246 composite particle Substances 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 150000002505 iron Chemical class 0.000 description 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005297 material degradation process Methods 0.000 description 1
- 239000013105 nano metal-organic framework Substances 0.000 description 1
- 239000013289 nano-metal-organic framework Substances 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 1
- 239000008055 phosphate buffer solution Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000979 synthetic dye Substances 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F3/00—Biological treatment of water, waste water, or sewage
- C02F3/34—Biological treatment of water, waste water, or sewage characterised by the microorganisms used
- C02F3/348—Biological treatment of water, waste water, or sewage characterised by the microorganisms used characterised by the way or the form in which the microorganisms are added or dosed
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/48—Treatment of water, waste water, or sewage with magnetic or electric fields
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12N—MICROORGANISMS OR ENZYMES; COMPOSITIONS THEREOF; PROPAGATING, PRESERVING, OR MAINTAINING MICROORGANISMS; MUTATION OR GENETIC ENGINEERING; CULTURE MEDIA
- C12N11/00—Carrier-bound or immobilised enzymes; Carrier-bound or immobilised microbial cells; Preparation thereof
- C12N11/14—Enzymes or microbial cells immobilised on or in an inorganic carrier
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/48—Treatment of water, waste water, or sewage with magnetic or electric fields
- C02F1/488—Treatment of water, waste water, or sewage with magnetic or electric fields for separation of magnetic materials, e.g. magnetic flocculation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/08—Nanoparticles or nanotubes
Definitions
- the invention belongs to the field of composite material preparation, in particular to a magnetic nanoparticle microorganism composite material with a core-shell structure and a preparation method thereof, and its application in azo dye processing.
- azo dyes have a wide range of applications in the fields of industry, papermaking, leather, cosmetics and foodstuffs.
- azo dyes due to improper use and poor supervision, azo dyes have a great impact on people's living environment, so how to deal with azo dyes have become the research hotspot.
- the adsorption method as a simple and direct, the adsorption effect of significant concern, but the high cost, as well as secondary pollution and low recycling impede its development. Therefore, looking for an economical and sustainable method has become a hot topic both at home and abroad.
- Biodegradation has the economic, environmental and sustainable advantages aroused people's attention, if the direct use of microorganisms to degrade the dye, the degradation is a longer time, the high concentrations of dyes will also affect the micro-organisms. Therefore, the simple use of microorganisms has been limited in practice.
- the present invention provides a magnetic nanoparticle microorganism composite material with a core-shell structure and a preparation method for azo dye treatment, magnetic nanoparticles are modified onto microorganisms in order to achieve local dye enrichment and separation effect, achieve the effect of efficient treatment of dye wastewater.
- a preparation method of magnetic nanoparticle microbial composite material with core-shell structure comprising the following steps:
- modified ferroferric oxide nanoparticles are sequentially reacted with ferric chloride and trimesic acid to prepare core-shell structured magnetic nanoparticles; said modified ferroferric oxide nanoparticles are sequentially reacted with ferric chloride and trimesic acid for 8 to 20 times;
- the core-shell structured magnetic nanoparticles are modified to the surface of microbial to prepare magnetic nanoparticle microbial composite with core-shell structure.
- the present invention also disclosed a preparation method of magnetic nanoparticle microbial composite material with core-shell structure, comprising the following steps:
- modified ferroferric oxide nano particles are sequentially reacted with ferric chloride and trimesic acid to prepare magnetic nanoparticles with core-shell structure; said modified ferroferric oxide nanoparticles are sequentially reacted with ferric chloride and trimesic acid for 8 to 20 times.
- the present invention also disclosed a preparation method of a modified ferroferric oxide nanoparticle, characterized in comprising the following steps: reacting a mixture of ferric chloride, sodium citrate, sodium acetate, and ethylene glycol at 180° C. to 200° C. for 8 to 10 hours to prepare ferroferric oxide nanoparticles; then dispersing the ferroferric oxide nanoparticles into an alcohol solution, then adding thioglycolic acid, and ultrasonically reacting to prepare modified ferroferric oxide nanoparticles.
- the core-shell structured magnetic nanoparticles are modified to the surface of the microorganism to obtain a composite material.
- the mass ratio of ferric chloride, sodium citrate and sodium acetate is 1:(1.5 to 2):10;
- the ferroferric oxide prepared by the invention is advantageous for subsequent modification, and at the same time, has a large specific surface area, which is favorable for the adsorption performance of the whole material.
- the mass ratio of ferroferric oxide nanoparticles and thioglycolic acid is 100:(1 to 2); the ultrasonic reaction is carried out at room temperature, ultrasonic reaction time is 6 to 7 hours. After ultrasonic reaction, the product is washed with ultrapure water and ethanol to prepare modified ferroferric oxide nanoparticles. After modification, the surface of the nanoparticle has a carboxyl group, and the carboxyl group is an essential group for the next layer self-assembly step. Conducive to self-assembly stability and success.
- the modified ferroferric oxide nanoparticles are sequentially placed in an ethanol solution of ferric chloride and trimesic acid, and after each reaction, ultrasonic treatment is performed, and after 8 to 20 times of reaction, the product is washed with ultrapure water and ethanol, and then dried to obtain core-shell structured magnetic nanoparticles.
- a porous nano-metal organic framework can be coated on the surface of the ferroferric oxide, and the structure has strong selective adsorption capacity, and the core-shell nanoparticles can also be used for magnetic separation.
- the core-shell magnetic nanoparticles are modified to the surface of the microorganism, and then the dye is adsorbed and degraded.
- the mass ratio of the magnetic nanoparticles to the microorganism is 1:(15 to 20)
- the core-shell magnetic nanoparticles are reacted with the microorganisms in a buffer solution for 12 hours, and then washed by centrifugation, followed by washing with a buffer solution to effect modification of the core-shell structured magnetic nanoparticles to the surface of the microorganism.
- the prepared magnetic core-shell nanoparticles are loaded on the surface of the microorganism to combine the adsorption and the biodegradation, and the respective advantages are fully utilized, thereby solving the disadvantages of the existing single microorganisms and the adsorption method. Therefore, the present invention further discloses the use of a magnetic nanoparticle composite material with core-shell structure in treating a dye, and discloses the above-mentioned magnetic nanoparticle with core-shell structure and the modified ferroferric oxide nanoparticle in preparing a dye treating agent, such as the treatment of dye wastewater.
- the method disclosed by the invention of modifying the core-shell magnetic nanoparticles into microorganisms has the advantages of low economic cost, easy availability of raw materials, safe and convenient operation, magnetic separation can be carried out to improve the degradation effect, and the dye can also be partially enriched in the process, so that the dye can be degraded efficiently and the advantages of the combination of adsorption and biological methods can be effectively exerted.
- FIG. 1 is SEM image of ferroferric oxide nanoparticles, core-shell structured magnetic nanoparticles, micro-organisms, and magnetic nano-particle microbial composites with a core-shell structure;
- FIG. 2 is TEM image of ferroferric oxide nanoparticles, core-shell structured magnetic nanoparticles, micro-organisms, and magnetic nano-particle microbial composites with a core-shell structure;
- FIG. 3 is a BET diagram of core-shell magnetic nanoparticles
- FIG. 4 is a thermogravimetric graph of core-shell magnetic nanoparticles
- FIG. 5 is a core-shell structure of the magnetic nanoparticle microbial composite material degradation effect diagram
- FIG. 6 shows the effect of degradation of free microorganisms
- FIG. 7 for the composite material cycle diagram and separation effect.
- Embodiment 1 is a diagrammatic representation of Embodiment 1:
- a preparation method of a magnetic nanoparticle microorganism composite material with a core-shell structure comprises the following steps:
- FIG. 1 is a SEM image of ferroferric oxide nanoparticles (a), core-shell structured magnetic nanoparticles (b), microorganisms (c), and magnetic nanoparticle-based microbial composites; It can be seen from the figure that the Fe 3 O 4 nanoparticles are spherical and uniformly distributed, at the same time, it can be seen that the surface of the modified core-shell magnetic nanoparticle becomes more rough, It's easier to load with microbes, it can be seen that the microorganisms are cylindrical, and the magnetic nanoparticles have been successfully loaded onto the surface of microorganisms, this is a crucial step toward degradation.
- FIG. 2 is a TEM image of the ferric oxide nanoparticles (a), the core-shell structure magnetic nanoparticles (b), the microorganisms (c), and the magnetic nanoparticle microorganism composite material (d);
- the modified ferroferric oxide nanoparticle become nucleation shell structure, this can increase its specific surface area, increase the adsorption of dyes, in the meantime, it can be seen that the composite nanoparticle of the core-shell structure has been successfully loaded onto the surface of the microorganism.
- FIG. 3 for the core-shell magnetic nanoparticles BET; It can be calculated from the figure, the specific surface area is 305.7 m 2 /g, descript that composite particles have a strong adsorption capacity.
- FIG. 4 is a thermogravimetric diagram of core-shell magnetic nanoparticles. As can be seen from the figure, the modified material above the ferroferric oxide is about 20%, and the stability of the composite material is 400° C.
- Embodiment 2 is a diagrammatic representation of Embodiment 1:
- FIG. 5 shows the degradation efficiency of a magnetic nanoparticle microorganism composite having a core-shell structure. It can be seen from the figure that when the initial concentrations were 25 mg per liter (a) and 50 mg per liter (b) respectively.
- the composite material of the present invention can complete the dye degradation in 15 hours and 25 hours.
- FIG. 6 is the degradation effect of free microorganisms, it can be seen that acidic oranges, which were initially at 25 mg per liter (left) and 50 mg per liter (right), were degraded over 20 and 36 hours.
- FIG. 7 shows the cycle performance and the separation effect of the magnetic nano-particle microbe composite with the core-shell structure. It can be seen that the magnetic nano-particle microbe composite has better degradation effect after repeated three times of magnetic separation.
- the composite disclosed in the present invention shows that the composite material has a strong capability of degrading dyes on microorganisms, has high degradation efficiency, and the production process is simple, convenient, economic and environmental, recyclable, etc., so in waste water treatment it will have a good application.
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- Bioinformatics & Cheminformatics (AREA)
- Wood Science & Technology (AREA)
- Zoology (AREA)
- Genetics & Genomics (AREA)
- Health & Medical Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Hydrology & Water Resources (AREA)
- Water Supply & Treatment (AREA)
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- General Engineering & Computer Science (AREA)
- General Health & Medical Sciences (AREA)
- Inorganic Chemistry (AREA)
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Abstract
Description
Claims (7)
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CN201711023310.5 | 2017-10-26 | ||
CN201711023310 | 2017-10-26 | ||
CN201711023310.5A CN107583621A (en) | 2017-10-26 | 2017-10-26 | Magnetic nano-particle microorganism composite with core shell structure and preparation method thereof with handled in azo dyes in application |
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US20190127252A1 US20190127252A1 (en) | 2019-05-02 |
US10800689B2 true US10800689B2 (en) | 2020-10-13 |
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CN110540642B (en) * | 2019-09-17 | 2021-12-07 | 齐鲁工业大学 | Preparation method and application of 2,4, 6-trichlorophenol magnetic molecularly imprinted composite material |
CN112409537B (en) * | 2020-12-01 | 2022-11-25 | 河南省商业科学研究所有限责任公司 | Preparation method of molecularly imprinted polymer for specifically recognizing sildenafil |
CN112537797B (en) * | 2020-12-07 | 2023-04-18 | 安徽师范大学 | Ferroferric oxide/carbon nano tube/sulfur-loaded composite material with one-dimensional chain-like core-shell structure, preparation method and application |
CN114177909A (en) * | 2021-11-26 | 2022-03-15 | 福建师范大学 | Magnesium-coconut shell carbon-ferroferric oxide composite material and preparation method thereof |
CN114426676B (en) * | 2021-12-20 | 2023-03-24 | 南京师范大学 | Magnetic iron-based MOF microbial carrier material and preparation method thereof |
CN114849650B (en) * | 2022-05-09 | 2023-03-10 | 南京大学 | Preparation method and application of dual-surface-characteristic magnetically-modified zirconium MOFs adsorbent |
CN117361732B (en) * | 2023-10-11 | 2024-04-05 | 中国海洋大学 | Multi-thorn-shaped magnetic micro-nano robot for sewage treatment and preparation method thereof |
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Non-Patent Citations (2)
Title |
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Liu et al., Advanced Materials Research, 2013, 631-632:490-493. * |
Sharma et al., Sci Rep., 2018, 8:14766 or pp. 1-11 as printed. * |
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US20190127252A1 (en) | 2019-05-02 |
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